Textile material and the production thereof



Patented Nov. 5, 1929 UNITED STATES PATENT OFFICE ROBINSON PERCY FOULDS,JOHN THOMPSON MARSH, AND FREDERICK CHARLES WOOD, OF MANCHESTER, ENGLAND,ASSIGNORS T0 TOOTAL BROADHURST LEE COM- IPANY LIMITED, OF MANCHESTER,ENGLAND, A BRITISH COMPANY TEXTILE MATERIAL AND THE PRODUCTION THEREOFNo Drawing. Application filed Noveiifber 2, 1928, Serial No. 316,871,and in Sweden November 7, 1927.

This application is a continuation in part of our copending applicationfiled November 21, 1927, Serial N 0. 234,901.

This invention relates to an improved textile material and theproduction thereof. It is concerned with the treatment of such textilematerials as cotton, silk, wool, ramie, jute, hemp, artificial silk,acetyl silk and linen, for example in the form of fabric or yarns. Theinvention may be applied to mixed fabrics.

The invention is particularly applied to cellulosic materials. Forexample, hitherto, one of the greatest defects of a fabric composedentirely of cotton has been the ease with which such fabric is creasedor crumpled when crushed or'folded under pressure in the hand. The samedisadvantage is present in the case of other materials such asartificial silk and linen; some materials such as wool are less readilycreased or crumpled. The object of the present invention is to rendertextile materials less susceptible to creasing "or crushing, whileretaining the suppleness of a woven or knitted textile fabric and theprocess is not limited to cellulosic fabrics since useful results can beobtained by its application to other fabrics.

Our invention consists broadly in a process of treating cellulosic orother yarns or fabrics which eliminates or materially reduces theirliability to crease or crush. Our invention further consists in theprocess by which this result can be obtained wherein final condensationor polymerization of a synthetic resin in presence of cellulosic orother yarns or fabrics is effected in such manner as to produce anon-crush effector to reduce markedly the extent to which the materialcrushes or crumples without tendering the material unduly. A fabric isregarded as exhibiting a non-crush effect or possessing little or nosusceptibility to crease or crumple when it shows no pronounced creasingon folding or crushing in the hand.

The method of preparation of the intermediate resin (where such is used)must be chosen according to the nature of the material to be treated.Thus some solutions containing free phenol would dissolve acetyl silk;other solutions would destroy hemp or jute, and so on. Again substantialquantities of strong acid are undesirable for cotton during the dryingstage hereafter described but permissive with Wool.

As regards cellulosic fabrics, it is believed to be novel to produce afabric which possesses the above described properties and the inventionincludes such a fabric broadly.

It has already been proposed to treat fabrics in the presence of afiller with a dilute solution of a synthetic resin, and then to complete the condensation of the resin on the fabric, with the object ofmaking the filler permanent to washing.

We prefer not to use a filler, at any rate unless in relatively smallquantity. More: over we have found that it is desirable to'use moreconcentrated solutions of the soluble resin or its components, and toavoid the use on cellulosic fibres of strong acids. Various proposalshave also been made to impregnate fabrics with synthetic resins forvarious purposes but not with the present object in view and such priorproposals do not contain the working instructions necessary to obtainour novel result.

In the present invention it is preferred to mercerize the materialpreferably with alkali, wash out the alkali and impregnate the'wetmaterial with the synthetic resin components. Alternatively thefabricsmaybe dried prior to impregnation provided that suitablemechanical treatment such as nipping between rollers is applied toensure penetration of the synthetic resin into the individual fibres ofthe yarn. If the material is dried it is preferable to wet out withwater before impregnation.

In general it is believed that the novel result is to be ascribed to thepresence of synthetic resin within the individual fibres of which theyarn is composed and to its absence in quantity from between the fibresor between the yarns. If much resin is present between the fibres, ahard or brittle product is obtained.

The use of phenols or substituted phenols as resin components isparticularly important though other resins can be used.

The following are examples whereby according to our invention fabrics ofcotton or linen may have imparted to them the property of not creasingor crumpling when folded or crushed in the hand without undue ten deringof the cloth and so that this property is not substantially destroyed bywashing.

Example 1 phenol, 100 parts of 40% formaldehyde, 4'

parts of potassium carbonate which have been boiled'together for 5minutes under a reflux condenser and rapidly cooled. I

' After impregnation with the reaction mixture, in a mangle, (the timeof impregnation and the number of the type of cloth used), the fabric issqueezed so as to retain roughly the same weight of liquor as formerlyand dried at a low temperature or at the temperature of the stenter. Itis finallyheated for 2 minutes at 170C. on drying tins or by othermeans, so as to insolubilize the resin and produce the requiredproperty. A soaping process is then applied to remove the excessreagents and after washing and drying, the treatment is complete.

It is obvious that other swelling agents than caustic soda can be used.Thus the invention includes the impregnation of fabrics which have beenswollen with sulphuric acid or other reagents and washed.

If desired, the fabric can be treated with I a current of hot gaseousformaldehyde.

, ate or sodium bicarbonate),

It has been found advantageous to blow a.

current of ammonia gas on to the fabric dur-. prevent ing each of thedrying processes to the formation of deep colour.

I I Other condensing agents may be employed,

e. g. carbonates (such as potassium carbon- 'or pyridine.- In thesecases it may be desired to boil the mixture for a longer time prior toimpregnation.

As an example of a'ifacid catalyst, we may use 4 per cent naphthalenesulphonic acid instead of caustic soda as a condensing agent,

but in such case I the intermediate product should be made slightlyalkaline prior to im pregnation.

. containing 5% The-semi-condensation product may be obtained withoutheating if desired; for example a solution of phenol and formaldehyde ofcaustic soda is allowed to stand in the cold for several days.

If the semi-condensation is" driven too far nips given may vary with e.g. by over-boiling, it may be corrected, up to a certain formaldehyde,or suitable organic solvents to keep the product in solution.

Dilute solutions may be used by employing a series of impregnations withlow-temperature drying after each impregnation for example, drying atabout 40 to 50 (3., and' finally heating until the desired effect isobtained e. g. at 180 C. for 3 to 5 minutes.

Example 2 173 grs. p. brom phenol 263 ccs. 40% formaldehyde 2% on totalWeight 62 N aOH.

Example 3 40 grs. O-chlorophenol 100 ccs. formaldehyde 40% 4 cos. N aOH63 Tw.

Example 4 (1 part by weight) and formalde- 0 solution,(2 parts) aremixed to- Urea hyde 40 gether and made slightly alkaline by the additionof hexamine or caustic soda. This mixture is refluxed at the boil for,3to 5 minutes and cooled quickly. Three parts of the mixture are dilutedand to 4% of glacial acetic wider the equivalent amount of any weak acidare added. I Mercerized cloth -which has been squeezed and" left dampafter the mercerizing process is run through the mixture and givenseveral nips between rollers. The fabric is dried at a low temperatureand the resin made insoluble by heating at 180 C. for 2 minutes on tinsor by other means.

We may add that whenusing urea formaldehyde resins, alkaline catalystsmay be used to obtain the "intermediate condensation product butfit'isvery desirable to use acid catalysts for the final condensation on with.1 part of water point by adding phenol, alkali I the fabric sinceotherwise the non-crush of feet will be less resistant to washing.

For phenol-formaldehyde resin, alkaline catalysts may be used in bothstages of the condensation. With these resins, we ma add smallquantities of reducing agents suc as the known formaldehyde sulphoxylatecompoundsto prevent development of colour in the fabric on drying and/orexposure to air and light.

Other resins acetone phenolormaldehyde resin may be mentioned as oneexample.

Ea'ample 5 Dissolve 95 parts by weight of dihydroxy diphenyl dimethylmethane (acetone-phenol condensation product) in 120 parts by weight ofhot formaldehyde, cool and add 12 parts by weight of caustic sodasolution (specific gravity 1.20).

Wet mercerized fabric is run through aqueous formaldehyde (1040%formaldehyde), squeezed and then run through the above bath withrepeated nipping between rollers. The cloth is dried at a low temperature e. g. 40 C. when further condensation occurs between the acetonephenol body and the formaldehyde and is then heated on drying tins at175 C. for 2 minutes. A soaping to remove excess reagents completes thetreatment and the cloth is finally dried in the usual manner.

The proportions of acetone phenol to formaldehyde may be varied.

,It will be understood that in forming the intermediate condensationproduct as also the synthetic resin, the process in either example, is,apart from details, broadly similar to the well-known methods ofobtaining such bodies, though we have selected certain conditions asadvantageous, especially as regards the nature and proportion ofcatalyst and the time and temperature of heating.

. There are however certain matters which must be kept in view in orderthat the novel result may be attained satisfactorily. In so far as thesynthetic resin adheres to and does not penetrate the fibre of thematerial of which the fabric is made it is believed that it isrelatively disadvantageous because suppleness of the fabric is therebydiminished without imparting the noncreasing or noncrumpling propertiesthereto. Care should accordingly be taken to mediate condensation pronot losing prematurely its solubility-that is to say becoming insolublebefore ithas been able to penetrate the fibre of the material of thefabric. For example, if the synthetic resin components are heatedtogether for a much longer time, or with a much greater quantity ofcatalyst, than is specified in the examples, we have given, it isdifiicult to obtain the best result. It will not be possible to preventsome of the ive the desired results andrevent the inter-- syntheticresin adhering to the surface of t e fibres. Care should also be ,taken'not to tender unduly the fabric in the formation of the synthetic resinand to this end a relatively high temperature for a relatively shorttime is employed in the last stages of the synthetic resin condensation.

General considerations In general the result of the treatment accordingto the invention is to produce a noncrush effect on the fabric withoutundue tendering of the fabric, which will resist washing to asubstantial extent. The fabric should retain the suppleness of a wovenor knitted textile fabric, that is it should be capable of use as adress material and can be draped about the human body or can fall intograceful folds. It must not be too stiff. The success of the treatmentis to be judged by physical rather than chemical tests.

It is important to. avoid the addition of too much resin to the fabricsince this would cause undue stiffness and in addition, the fabric wouldbe liable to crease. This stiffness depends not only on the amount ofresin but also on other factors such as the method of its application,the extent to which it has been condensed before application andespecially its distribution within the fabric. It is preferable tomercerize the fabric before impregnation and the mercerization must bewell done.

Mechanical treatment e. g. pressure, is desirable during impregnationand especially when treating unmercerized fabric, to secure the desireddistribution.

We have described the novel results obtained and we have given examplesby which the process can be successfully performed. In varying theseexamples the final product must be tested by comparison with theoriginal cloth and special attention must be paid to standardizing theworking conditions, especially those relating to the extent ofcondensation at each stage, e. g. the time, temperature, dilution, andnature of catalyst. The fabrics must be treated, if necessary, so thatthey will be readily wetted-out by the impregnating solutions.

It will be clear that the invention is not limited to the details shownin the examples since in the light of our disclosure these examples maybe considerably modified, provided that the specified physical resultsare obtained.

We declare that what we claim is 1. An impregnated textile material produced by the process of claim 7 in which so much of an impregnatingagent, solidified from a liquid, is contained within but notsubstantially between the individual fibers that the material shows asubstantially lessened tendency to crease or crumple While retaining itssuppleness.

2. An impregnated cellulosic material produced by the process of claim 7in which so much of an impregnating agent, solidified from a liquid, iscontained within but substantially not between the individual-fibersthat the material shows a substantially'lessened tendency to crease orcrulnple while retaining its suppleness.

3. A cellulosic textile fabric produced by the process of claim 9 inwhich so much' of a synthetic resin, solidified from a 1i ui'd;contained within but not substantia ly between the individual fibersthat the fabric is supple but shows a substantially lessened tent encyto crease or crumple.

4. An impregnated textile material produced by the process of claim 9containing within but not substantially between theindividual fibers asynthetic resin which is completely insolubilized by heating and in suchquantity that the material shows a substantially lessened tendency tocrease or crumpie while retaining its suppleness.

5. A textile fabric produced by the process of cIaim 11 containingwithin but not substantially between the individual fibersso muchphenol-formaldehyde synthetic resin solidified from a liquid that thefabric is supple but shows a substantially lessened tendency to creaseor crumple.

6. Animpregnated fabric produced by the process of claim 7 in which theindividual fibers are filled with so much of an agent solidified from aliquid thatthey become re- 3 silient and thereby impart to the fabricthe ing out the swelling agent, impregnating the material with a liquidcomprising a solidifiable agent, removing the impregnating agent, ifany,from betweenlthe fibres, and solidifying the impregnating agent. 1

9. The process of rendering a textile ma terial substantially lessliable to creasing or crumpling without substantially lessening itssuppleness, which comprises impregnating the individual fibres with anintermediate condensation product of a synthetic resin, re-

' moving said intermediate condensation product, if any, from betweenthe fibres, and heating the material to such an extent as to completelyinsolubilize the resin.

10. The process of rendering a cellulosic textile material substanti llyless liable'to creasing or cruinpling witiiout substantially lessening.its suppleness, which comprises treating the material with caustic sodaof mercerizing strength,- washing out the caustic.

soda, impregnating the individual fibres-with an intermediatecondensation product of a synthetic resin,- removing said intermediatecondensation product, if any, from between the.-'fibres, and heating thematerial to completely insolubilize the resin.

11;: The process of rendering a textile material substantially lessliable to creasing or crumpling' without substantially lessening itssuppleness, which] comprises impregnating the individual fibres-with anintermediate condensationproduct of a phenol-formaldehyde resin,removing said intermediate condensation product,.-if any, from betweenthe fibres, and heating the material; for a. short time at atemperaturenot less than about 160 F. to completely insolubilize the resin.

12. The process as in claim 9 in which a cellulosic material isimpregnated with a phenolformaldehyde resin and "the resin is finallycondensed by heating in presence of an alkaline catalyst. I

13. The process as in claim? in which the textile material is subjectedto mechanical treatment while wet with the impregnating liquid, toassist inithe desired distribution of the solidifiable agent.

-' 14. The process as in claim-7 in which a cot ton fabric is mercerizedbefore impregnation.

15. The-processas inclaim 9 in which a concentrated solution is used forimpregnation. In witness whereof, we have hereunto signed our names this20th day of October, 1928.

ROBINSON PERCY FOULDS. JOHN THOMPSON MARSH. FREDERICK CHARLES WOOD.

